Kiang C H, Campos-Flor S, Inturrisi C E
J Chromatogr. 1981 Jan 2;222(1):81-93. doi: 10.1016/s0378-4347(00)81035-x.
A method is described for the simultaneous determination of 1, alpha-acetylmethadol (LAAM) and five active metabolites--noracetylmethadol, dinoracetylmethadol, methadol, normethadol, and dinormethadol--in biofluids by high-performance liquid chromatography using a normal-phase column and a UV detector at 218 nm. The compounds are recovered from biofluids by a multistep liquid--liquid extraction. The mobile phase is methanol--acetonitrile (70:30, v/v) containing 0.015% ammonium hydroxide as the modifier. Retention times can be varied by adjusting the composition of the mobile phase to maximize peak height for quantitation using l-propranolol as the internal standard or peak separation for the collection of fractions. Using a UV detector the lower limit of sensitivity is 10 ng/ml of biofluid. Using fraction collection of radiolabeled drug and metabolites followed by liquid scintillation counting the lower limit of sensitivity is 1.0 ng/ml. Commonly used or abused narcotics including morphine, heroin, meperidine, methadone and propoxyphene do not interfere with the analysis. The method has been applied to plasma and urine samples from humans, sheep and rats. Extracts of urine from patients receiving maintenance treatment with LAAM contain LAAM and each of the five active metabolites.
本文描述了一种采用正相柱和218 nm紫外检测器，通过高效液相色谱法同时测定生物流体中1-α-乙酰美沙醇（LAAM）及其五种活性代谢物——去甲乙酰美沙醇、双去甲乙酰美沙醇、美沙醇、去甲美沙醇和双去甲美沙醇的方法。这些化合物通过多步液-液萃取从生物流体中回收。流动相为含有0.015%氢氧化铵作为改性剂的甲醇-乙腈（70:30，v/v）。通过调整流动相组成可改变保留时间，以使用l-普萘洛尔作为内标时最大化峰高进行定量，或为收集馏分实现峰分离。使用紫外检测器时，生物流体的灵敏度下限为10 ng/ml。采用放射性标记药物及其代谢物的馏分收集，随后进行液体闪烁计数时，灵敏度下限为1.0 ng/ml。包括吗啡、海洛因、哌替啶、美沙酮和丙氧芬在内的常用或滥用麻醉药品不干扰分析。该方法已应用于来自人类、绵羊和大鼠的血浆和尿液样本。接受LAAM维持治疗患者的尿液提取物中含有LAAM及其五种活性代谢物中的每一种。
